JP2003277812A - Platinum powder - Google Patents
Platinum powderInfo
- Publication number
- JP2003277812A JP2003277812A JP2002124963A JP2002124963A JP2003277812A JP 2003277812 A JP2003277812 A JP 2003277812A JP 2002124963 A JP2002124963 A JP 2002124963A JP 2002124963 A JP2002124963 A JP 2002124963A JP 2003277812 A JP2003277812 A JP 2003277812A
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- Japan
- Prior art keywords
- platinum
- powder
- metal compound
- fine
- platinum powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、白金微粉末、又は
加熱されることにより分解されるかあるいは還元される
ことにより白金微粉末になる白金化合物の微粉末とアル
カリ金属化合物又はアルカリ土類金属化合物の1種又は
それ以上と混合した後、加熱処理することによって、任
意の粒径の白金粉末を再現性良好に、経済的に提供する
ことに関する。TECHNICAL FIELD The present invention relates to a fine platinum powder, or a fine platinum compound powder which becomes a fine platinum powder when decomposed or reduced by heating and an alkali metal compound or an alkaline earth metal. The present invention relates to providing platinum powder of any particle size with good reproducibility and economically by mixing with one or more compounds and then subjecting to heat treatment.
【0002】[0002]
【従来の技術】従来、一般に金属粉末を得る場合、所望
する金属の原料となる金属を所望の数量に従って溶解炉
に投入し、金属の原料金属の融点以上に加熱して溶解混
合し、該溶解混合物を空気中又は液中に霧状に噴霧する
ことによって得られてきた。しかし、白金の融点は空気
中では1774℃と高温であり、白金を空気中で溶解さ
せるには通常1900℃以上の高温で溶解させなければ
ならず、空気中の溶解に関しては困難であり、溶解させ
るためには真空中で溶解させなければならないなど、大
規模の装置を必要としなければならなかった。また、溶
解した後でも、真空中の溶解物を大気中や水中に噴霧す
ることは装置としても困難であり、製造装置が大規模に
ならざるを得なかった。そのため、粒子形状も安定した
物は得られなかった。2. Description of the Related Art Conventionally, when a metal powder is generally obtained, a metal as a raw material of a desired metal is charged into a melting furnace in accordance with a desired quantity, heated to a temperature not lower than a melting point of the metal of the raw material, mixed and melted. It has been obtained by atomizing the mixture in air or liquid. However, the melting point of platinum is as high as 1774 ° C. in air, and in order to dissolve platinum in air, it is usually necessary to dissolve it at a high temperature of 1900 ° C. or higher, which is difficult to dissolve in air. In order to do so, it was necessary to use a large-scale apparatus such as melting in a vacuum. Further, even after melting, it is difficult to spray the melted material in vacuum into the air or water, and the manufacturing apparatus has to be large scale. Therefore, a particle having a stable particle shape could not be obtained.
【0003】[0003]
【発明が解決しようとする課題】従来の方法では、白金
粉末を得る場合、1900℃以上の高温で溶解し、大気
中又は液中に噴霧分散させることが必要であるが、真空
中で溶解して、無理に大気中又は液中に噴霧分散させな
ければならず、大がかりで特別の装置が必要となり、常
に安定した所望の粒度形状の白金粉末が得にくい状況で
あった。そこで、本発明は常に所望の粒子形状の白金粉
末を得ることができる方法を提供することにある。In the conventional method, when platinum powder is obtained, it is necessary to melt it at a high temperature of 1900 ° C. or higher and spray-disperse it in the air or in a liquid. Therefore, it is necessary to forcibly disperse the particles in the air or in the liquid, which requires a large-scale special device, and it is difficult to always obtain a stable platinum powder having a desired particle size. Therefore, the present invention is to provide a method capable of always obtaining a platinum powder having a desired particle shape.
【0004】[0004]
【課題を解決するための手段】本発明者は白金粉末の制
御に関して鋭意研究の結果所望の粒度、形状の白金粉末
を得ることを見いだし、本発明に至った。本発明は、白
金微粉末又は、加熱されることにより分解されるか、又
は還元されることにより白金微粉末になる白金化合物と
アルカリ金属化合物又はアルカリ土類金属化合物の1種
又はそれ以上と混合した後、加熱処理することによって
常に所望の粒子形状の白金粉末を安定して得ることにか
かるものである。Means for Solving the Problems As a result of intensive studies on control of platinum powder, the present inventor has found that a platinum powder having a desired particle size and shape can be obtained, and completed the present invention. The present invention relates to a fine platinum powder, or a platinum compound which is decomposed by heating or reduced to become fine platinum powder, and one or more kinds of alkali metal compounds or alkaline earth metal compounds. After that, heat treatment is performed to always obtain a stable platinum powder having a desired particle shape.
【0005】[0005]
【発明の実施の形態】以下、本発明について詳しく説明
する。本発明は白金微粉末、加熱されることにより分解
されるか還元されることにより白金微粉末になる白金化
合物とアルカリ金属化合物又はアルカリ土類金属化合物
の1種又はそれ以上と混合した後、当該混合物を加熱処
理を行うことにある。BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below. The present invention relates to a fine platinum powder, a platinum compound which is decomposed by heating or becomes a fine platinum powder by reduction, and one or more of an alkali metal compound or an alkaline earth metal compound, The mixture is subjected to heat treatment.
【0006】本発明に用いられる白金微粉末としては、
白金ブラック、白金スポンジ、加熱されることにより分
解されるか、あるいは還元されることによって白金微粉
末になる酸化白金、ジクロロテトラアンミン白金、ジニ
トロジアンミン白金及びその硝酸塩、テトラクロロヘキ
サアンミン白金、ヘキサヒドロキソ白金酸及びその硝酸
塩、ヘキサヒドロキソ白金酸ナトリウムなどの有機白金
化合物、塩化白金酸、塩化白金酸カリウムなどが挙げら
れる。上記白金微粉末の粒径は、特に制限はないが、好
ましくは1nm〜10000nm程度の粒径が適してい
る。The platinum fine powder used in the present invention includes:
Platinum black, platinum sponge, platinum oxide that is decomposed or reduced by heating to become fine platinum powder, dichlorotetraammineplatinum, dinitrodiammineplatinum and its nitrate, tetrachlorohexaammineplatinum, hexahydroxoplatinum Examples thereof include acids and nitrates thereof, organic platinum compounds such as sodium hexahydroxoplatinate, chloroplatinic acid, potassium chloroplatinate, and the like. The particle size of the platinum fine powder is not particularly limited, but a particle size of about 1 nm to 10000 nm is suitable.
【0007】本発明に用いられるアルカリ金属化合物と
しては、Li、Na、K、Rb、Csの酸化物、水酸化
物、炭酸塩、硫酸塩、硝酸塩、塩化物、有機酸塩などが
挙げられる。又、アルカリ土類金属化合物としては、B
e、Mg、Ca、Sr、Ba、Raの酸化物、水酸化
物、炭酸塩、硫酸塩、硝酸塩、塩化物、有機酸塩などが
挙げられる。Examples of alkali metal compounds used in the present invention include oxides, hydroxides, carbonates, sulfates, nitrates, chlorides and organic acid salts of Li, Na, K, Rb and Cs. Further, as the alkaline earth metal compound, B
Examples thereof include oxides, hydroxides, carbonates, sulfates, nitrates, chlorides and organic acid salts of e, Mg, Ca, Sr, Ba and Ra.
【0008】これらアルカリ金属化合物、アルカリ土類
金属化合物の1種又はそれ以上と混合される。It is mixed with one or more of these alkali metal compounds and alkaline earth metal compounds.
【0009】混合する場合の混合装置としては、一般に
ボールミル、アトライター、遊星ボールミル、などを用
いても良いが、ボールミルなどを用いた場合、白金微粉
末が、偏平やフレーク状になる恐れがある。上記のおそ
れがある場合には、1000rpm以上の高速撹拌装置
で混合する場合がある。1000rpm以上の高速攪拌
装置の例としてはスーパーミキサー、ヘンシェルミキサ
ーなどがあげられる。Generally, a ball mill, an attritor, a planetary ball mill, or the like may be used as a mixing device for mixing, but when a ball mill or the like is used, the platinum fine powder may become flat or flaky. . When there is a possibility of the above, mixing may be performed with a high speed stirring device of 1000 rpm or more. Examples of the high speed stirring device of 1000 rpm or more include a super mixer and a Henschel mixer.
【0010】混合機、撹拌装置でよく混合分散した混合
物は、加熱処理される。加熱処理は非酸素雰囲気下で行
うのが望ましい。非酸素雰囲気とは、アルゴン、窒素、
水素、又は窒素、水素の混合ガス雰囲気である。非酸素
雰囲気で加熱することにより、白金化合物は還元され
て、白金微粉末にする。The mixture well mixed and dispersed by a mixer and a stirring device is heat-treated. The heat treatment is preferably performed in a non-oxygen atmosphere. Non-oxygen atmosphere means argon, nitrogen,
It is an atmosphere of hydrogen or a mixed gas of nitrogen and hydrogen. By heating in a non-oxygen atmosphere, the platinum compound is reduced to platinum fine powder.
【0011】加熱処理を行う過程で、白金微粒子は、接
触している金属粉末同士が、粒成長するが、介在してい
るアルカリ金属化合物、アルカリ土類金属化合物のため
に粒成長が阻害される。そのため、比較的粒度の小さい
白金粉末を得るためには、混合するアルカリ金属化合
物、アルカリ土類金属化合物を多量に混合すればよい。
このようにして、アルカリ金属化合物、アルカリ土類金
属化合物の添加量の多少によって、任意の粒度の白金粉
末を得ることが出来る。また加熱処理温度、加熱処理時
間条件によっても白金粉末の粒度が影響される。加熱処
理温度は制限がないが、一般には1,500℃以下が望
ましい。また、加熱処理時間は制限がないが、所望の白
金の粒度により決定される。In the process of heat treatment, the platinum fine particles cause grain growth between the metal powders in contact with each other, but the grain growth is hindered by the intervening alkali metal compound or alkaline earth metal compound. . Therefore, in order to obtain a platinum powder having a relatively small particle size, a large amount of the alkali metal compound and the alkaline earth metal compound to be mixed may be mixed.
In this way, a platinum powder having an arbitrary particle size can be obtained depending on the amounts of the alkali metal compound and the alkaline earth metal compound added. The particle size of the platinum powder is also affected by the heat treatment temperature and heat treatment time conditions. The heat treatment temperature is not limited, but generally 1,500 ° C. or lower is desirable. Although the heat treatment time is not limited, it is determined by the desired particle size of platinum.
【0012】高温で、長時間の加熱時間を保つほど白金
粉末の粒度が大きくなり、逆に低温で短時間の加熱では
白金粉末の粒度は小さくなる。The particle size of the platinum powder increases as the heating time is maintained at a high temperature for a long time, and conversely, the particle size of the platinum powder decreases when heated at a low temperature for a short time.
【0013】加熱終了後、加熱処理物を水中や硝酸、硫
酸等の水溶液中に投入して、アルカリ金属化合物、アル
カリ土類金属化合物を除去する。最後に充分に水洗いを
行い、濾過、乾燥させて、白金粉末を得る。After completion of heating, the heat-treated product is put into water or an aqueous solution of nitric acid, sulfuric acid or the like to remove the alkali metal compound and the alkaline earth metal compound. Finally, it is thoroughly washed with water, filtered and dried to obtain platinum powder.
【0014】[0014]
【実施例】次に、実施例を挙げて本発明を説明するが、
本発明は以下の例のみに限定されるものではない。EXAMPLES Next, the present invention will be described with reference to examples.
The present invention is not limited to the following examples.
【0015】[実施例1]白金ブラック微粉末(粒子径
約100nm)100重量部と炭酸カリウム微粉末40
0重量部とをスーパーミキサーに入れて充分に混合分散
させた。次に、この混合体を還状炉(電気炉)の中に入
れて、窒素ガスを流しながら1250℃で加熱した後に
850℃まで下げて加熱した。その後、この加熱処理し
た混合体を水中に投入し、分散させた後に濾過し、濾過
物を硝酸水溶液中に投入し、さらに水洗後、乾燥させ
て、白金粉末を得た。得られた白金粉末は、粒子径約
1.4μmであった。Example 1 100 parts by weight of platinum black fine powder (particle diameter of about 100 nm) and potassium carbonate fine powder 40
0 part by weight was placed in a super mixer and thoroughly mixed and dispersed. Next, this mixture was put into a return furnace (electric furnace), heated at 1250 ° C. while flowing nitrogen gas, and then lowered to 850 ° C. and heated. Then, this heat-treated mixture was put into water, dispersed and filtered, and the filtered product was put into an aqueous nitric acid solution, further washed with water and dried to obtain a platinum powder. The obtained platinum powder had a particle size of about 1.4 μm.
【0016】[実施例2]白金ブラック微粉末(粒子径
約100nm)100重量部と炭酸カリウム微粉末10
0重量部とをスーパーミキサーに入れて充分に混合分散
させた。次にこの混合体を還状炉(電気炉)にいれて窒
素ガスを流しながら1200℃で加熱した。その後、こ
の加熱処理した混合体を水中に投入し、分散させた後に
濾過し、濾過物を硝酸水溶液中に投入し、さらに水洗後
乾燥させて白金粉末を得た。得られて白金粉末は粒子径
約2.5μmであった。Example 2 100 parts by weight of platinum black fine powder (particle diameter of about 100 nm) and potassium carbonate fine powder 10
0 part by weight was placed in a super mixer and thoroughly mixed and dispersed. Next, this mixture was placed in a return furnace (electric furnace) and heated at 1200 ° C. while flowing nitrogen gas. Then, this heat-treated mixture was put into water to disperse it, followed by filtration. The filtered product was put into an aqueous nitric acid solution, further washed with water and dried to obtain a platinum powder. The obtained platinum powder had a particle size of about 2.5 μm.
【0017】[実施例3]白金ブラック微粉末(粒子径
約100nm)100重量部と炭酸マグネシウム微粉末
400重量部とをスーパーミキサーに入れて充分に混合
分散させた。次にこの混合体を還状炉(電気炉)にいれ
て窒素ガスを流しながら1250℃で加熱した後に、8
50℃まで下げて加熱した。その後、この加熱処理した
混合体を水中に投入し、分散させた後に濾過し、濾過物
を硝酸水溶液中に投入し、さらに水洗後乾燥させて白金
粉末を得た。得られた白金粉末は粒子径約1.5μmで
あった。Example 3 100 parts by weight of platinum black fine powder (particle diameter of about 100 nm) and 400 parts by weight of magnesium carbonate fine powder were put in a super mixer and sufficiently mixed and dispersed. Next, after putting this mixture in a return furnace (electric furnace) and heating at 1250 ° C. while flowing nitrogen gas,
It was lowered to 50 ° C. and heated. Then, this heat-treated mixture was put into water to disperse it, followed by filtration. The filtered product was put into an aqueous nitric acid solution, further washed with water and dried to obtain a platinum powder. The obtained platinum powder had a particle size of about 1.5 μm.
【0018】[実施例4]実施例2の中で、炭酸カリウ
ム微粉末100重量部を炭酸バリウム100重量部に変
えた他は、全て同じ条件で操作を行い、白金粉末を得
た。得られた白金粉末は粒子径約2.3μmであった。Example 4 Platinum powder was obtained in the same manner as in Example 2, except that 100 parts by weight of fine potassium carbonate powder was changed to 100 parts by weight of barium carbonate. The platinum powder obtained had a particle size of about 2.3 μm.
【0019】[実施例5]実施例1の中で、炭酸カリウ
ム微粉末400重量部を水酸化カルシウム400重量部
に変えた他は、全て同じ条件で操作を行い、白金粉末を
得た。得られた白金粉末は粒子径約1.7μmであっ
た。[Example 5] Platinum powder was obtained by the same procedure as in Example 1 except that 400 parts by weight of potassium carbonate fine powder was changed to 400 parts by weight of calcium hydroxide. The platinum powder obtained had a particle size of about 1.7 μm.
【0020】[実施例6]白金微粉末(粒子径約100
nm)100重量部と水酸化カルシウム微粉末400重
量部とをスーパーミキサーに入れて充分に混合分散させ
た。次にこの混合体を還状炉(電気炉)にいれて窒素ガ
ス、水素ガスを流しながら1200℃で加熱した後に、
当該混合物を水中に投入し、分散させた後濾過し、濾過
物を硝酸水溶液中に投入し、さらに水洗後濾過、乾燥さ
せて白金粉末を得た。得られた白金粉末は粒子径約1.
8μmであった。[Example 6] Platinum fine powder (particle size: about 100)
(100 nm) and 400 parts by weight of calcium hydroxide fine powder were put in a super mixer and sufficiently mixed and dispersed. Next, after putting this mixture in a return furnace (electric furnace) and heating at 1200 ° C. while flowing nitrogen gas and hydrogen gas,
The mixture was put into water, dispersed and filtered, the filtered product was put into a nitric acid aqueous solution, further washed with water, filtered, and dried to obtain a platinum powder. The obtained platinum powder has a particle size of about 1.
It was 8 μm.
【0021】[実施例7]酸化白金(粒子径約100n
m)100重量部と炭酸カリウム微粉末500重量部と
をスーパーミキサーに入れて充分に混合分散させた。次
にこの混合体を還状炉(電気炉)にいれて窒素ガス、水
素ガスを流しながら1200℃で加熱した後に、当該混
合物を水中に投入し、分散させた後に濾過し、濾過物を
硝酸水溶液中に投入し、さらに水洗後濾過乾燥させて白
金粉末を得た。得られた白金粉末は粒子径約1.8μm
であった。Example 7 Platinum oxide (particle size: about 100 n
m) 100 parts by weight and 500 parts by weight of potassium carbonate fine powder were put into a super mixer and sufficiently mixed and dispersed. Next, this mixture is put into a return furnace (electric furnace) and heated at 1200 ° C. while flowing nitrogen gas and hydrogen gas, and then the mixture is put into water, dispersed and filtered, and the filtered product is nitric acid. It was put into an aqueous solution, further washed with water, filtered and dried to obtain a platinum powder. The obtained platinum powder has a particle size of about 1.8 μm.
Met.
【0022】[0022]
【発明の効果】本発明によって、白金粉末を合成する場
合に、比較的低温で任意の粒子径の白金粉末を合成可能
になる。さらに当該白金粉末は粒子径がアルカリ金属化
合物、アルカリ土類金属化合物の添加量、加熱温度によ
って安定して合成可能である。さらに当該白金粉末は、
粒子径がほぼ均一に合成可能である。According to the present invention, when synthesizing platinum powder, it becomes possible to synthesize platinum powder having an arbitrary particle size at a relatively low temperature. Further, the platinum powder can be stably synthesized with a particle size depending on the addition amount of the alkali metal compound or the alkaline earth metal compound and the heating temperature. Furthermore, the platinum powder is
It is possible to synthesize particles having a substantially uniform particle size.
Claims (4)
ルカリ土類金属化合物の1種又はそれ以上と混合した
後、当該混合物を加熱処理してなる白金粉末。1. A platinum powder obtained by mixing fine platinum powder with one or more of an alkali metal compound or an alkaline earth metal compound, and then heat-treating the mixture.
いは還元されることにより白金微粉末になる白金化合物
の微粉末にアルカリ金属化合物又はアルカリ土類金属化
合物の1種又はそれ以上と混合した後、当該混合物を加
熱処理してなる白金粉末。2. A fine powder of a platinum compound which is decomposed by heating or reduced into a fine platinum powder is mixed with one or more kinds of an alkali metal compound or an alkaline earth metal compound. Then, a platinum powder obtained by heating the mixture.
解されるか又は還元されることにより白金微粉末になる
白金化合物の微粉末にアルカリ金属化合物又はアルカリ
土類金属化合物の1種又はそれ以上と混合した後、当該
混合物を加熱処理してなる白金ロジウム合金微粉末。3. Platinum fine powder, or a fine powder of a platinum compound which becomes a fine platinum powder when decomposed or reduced by heating, and one or more of an alkali metal compound or an alkaline earth metal compound. Platinum-rhodium alloy fine powder obtained by heating the mixture after mixing with the above.
解されるか又は還元されることにより白金微粉末になる
白金化合物の微粉末と、アルカリ金属化合物又はアルカ
リ土類金属化合物の1種又はそれ以上とを1000rp
m以上の高速撹拌装置で混合した後、加熱処理をした後
にアルカリ金属化合物又はアルカリ土類金属化合物、又
はアルカリ金属化合物又はアルカリ土類金属化合物の分
解物を除去してなる白金粉末の製造方法。4. Platinum fine powder, or a fine powder of a platinum compound which becomes a fine platinum powder when decomposed or reduced by heating, and one of an alkali metal compound or an alkaline earth metal compound, or 1000 rp and above
A method for producing platinum powder, which comprises mixing with a high-speed stirring device of m or more and then heat-treating and then removing an alkali metal compound or an alkaline earth metal compound or a decomposed product of the alkali metal compound or an alkaline earth metal compound.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002124963A JP2003277812A (en) | 2002-01-15 | 2002-03-25 | Platinum powder |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002-40777 | 2002-01-15 | ||
JP2002040777 | 2002-01-15 | ||
JP2002124963A JP2003277812A (en) | 2002-01-15 | 2002-03-25 | Platinum powder |
Publications (1)
Publication Number | Publication Date |
---|---|
JP2003277812A true JP2003277812A (en) | 2003-10-02 |
Family
ID=29253499
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP2002124963A Pending JP2003277812A (en) | 2002-01-15 | 2002-03-25 | Platinum powder |
Country Status (1)
Country | Link |
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JP (1) | JP2003277812A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006322051A (en) * | 2005-05-19 | 2006-11-30 | Noritake Co Ltd | Metal powder, and method for producing the same |
DE102009017346A1 (en) | 2008-04-10 | 2009-10-15 | Yamamoto Precious Metal Co. Ltd. | Process for the preparation of fine precious metal particles |
JP2011162868A (en) * | 2010-02-15 | 2011-08-25 | Yamamoto Precious Metal Co Ltd | Method for manufacturing noble metal fine particle |
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2002
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006322051A (en) * | 2005-05-19 | 2006-11-30 | Noritake Co Ltd | Metal powder, and method for producing the same |
DE102009017346A1 (en) | 2008-04-10 | 2009-10-15 | Yamamoto Precious Metal Co. Ltd. | Process for the preparation of fine precious metal particles |
JP2011162868A (en) * | 2010-02-15 | 2011-08-25 | Yamamoto Precious Metal Co Ltd | Method for manufacturing noble metal fine particle |
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